(S)-卡巴拉汀D-(+)-DTTA盐的合成与晶体结构

Synthesis and crystal structure of (S)-rivastigmine D-(+)-DTTA

标题化合物由3-(1-二甲氨基乙基)苯酚与N-乙基-N-甲基氨基甲酰氯反应合成卡巴拉汀游离碱,再与(+)-O,O′-二对甲基苯甲酰-D-酒石酸(D-(+)-DTTA)成非对映体盐制得。它的晶体结构已通过单晶X-射线衍射测试得到确定。通过对3477个可以观察到的独立衍射点[I>2σ(I)]的测试,结果表明:该晶体属于斜方晶系,P21212空间群,a=14.6084(7),b=30.7876(14),c=7.5442(3),α=90,β=90,γ=90,V=3393.1(3)3,Z=2,Dc=1.246mg/m3,μ=0.092mm-1,F(000)=1352,R=0.0529,wR=0.1459。

The compound （ S）-rivastigmine D- （ ＋ ）-DTTA （ [ C34 H40N2O10], Mr = 636.27） was synthesized by the reaction of 3- （ 1-dimethylaminoethyl ）-phenol with N-ethyl-N-methylcar- bamoylchlofide, followed by preparation of the diastereoisomeric salt with （ ＋ ）-O, O＇-di-（p-toluoyl）-D-tartaric acid （D-（ ＋ ）- DTTA）. Its crystal structure was determined by the single-crystal X-ray diffraction method. The crystal was of an orthorhombic system,with a space group of P21 21 2 having the following parameters： a = 14.608 4 （7）A, b = 30.787 6 （14）A, c = 7.544 2（3）A, α = 90,β = 90, γ = 90, V = 339 3. 1（3）A^3, Z = 2,Dc = 1.246 Mg/m^3, μ =0.092 mm^-1, F（000） = 1 352,R = 0.052 9 and wR = 0.1459.